Simultaneous Determination of Nine Quinolones in Pure Milk Using PFSPE-HPLC-MS/MS with PS-PAN Nanofibers as a Sorbent

In this study, a packed-fiber solid-phase extraction (PFSPE)-based method was developed to simultaneously detect nine quinolones, including enrofloxacin (ENR), ciprofloxacin (CIP), ofloxacin (OFL), pefloxacin (PEF), lomefloxacin (LOM), norfloxacin (NOR), sarafloxacin (SAR), danofloxacin (DAN), and difloxacin (DIF), in pure milk, using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Polystyrene (PS) and polyacrylonitrile (PAN) were combined to form PS-PAN composite nanofibers through electrospinning. The nanofibers were used to prepare the home-made extraction columns, and the process was optimized and validated using blank pure milk. The analytical method showed high accuracy, and the recoveries were 88.68-97.63%. Intra-day and inter-day relative standard deviations were in the ranges of 1.11-6.77% and 2.26-7.17%, respectively. In addition, the developed method showed good linearity (R-2 >= 0.995) and low method quantification limits for the nine quinolones (between 1.0-100 ng/mL) for all samples studied. The nine quinolones in the complex matrix were directly extracted using 4.0 mg of PS-PAN composite nanofibers as a sorbent and completely eluted in 100 mu L elution solvent. Therefore, the developed PFSPE-HPLC-MS/MS is a sensitive and cost-effective technique that can effectively detect and control nine quinolones in dairy products.

Automated summary

In this study, a sensitive and cost-effective method combining packed-fiber solid-phase extraction and high-performance liquid chromatography coupled with tandem mass spectrometry was developed for simultaneous detection of nine quinolones in pure milk. The method showed high accuracy, good linearity, and low method quantification limits.